摘要
建立鸡肉中硝基呋喃类药物代谢物残留的液相色谱-串联质谱检测方法。样品经盐酸水解,邻硝基苯甲醛过夜衍生,调pH 7.2后,用乙酸乙酯提取,正己烷净化,以多离子反应检测模式(MRM)进行测定,采用同位素内标法进行定量。结果表明,该方法的线性范围为0.5～10μg/kg, 4种代谢物的线性相关系数均不小于0.999 4,检出限为0.5μg/kg。在0.5, 1.0和5.0μg/kg的添加水平下,加标回收率为85.6%～105.2%, RSD为4.17%～5.45%(n=6)。该法可作为鸡肉中4种硝基呋喃类药物的代谢物残留量同时分析的有效手段。
An analytical method was developed for the determination of metabolites of nitrofuran antibiotics in chicken by using ultra performance liquid chromatography coupled with tandem mass spectrometry. The samples were hydrolyzed with HCl. The derivative solutions were adjusted to pH 7.2, and the analytes were extracted byethylacetate. The analytes were detected by tandem mass spectrometry with electrospray ionization source with multiple reaction monitoring(MRM) mode. The developed method showed a good linear correlation between the peak area ratios of the analyte and the internal standard and the concentration of the analyte with the correlation coefficients which were all above 0.999 4 and over the dynamic range of 0.5-10 μg/kg. The limits of quantitation(LOQs) of AOZ, AMOZ, SEM and AHD were 0.5 μg/kg. The average recoveries of all the compounds at four spiked levels of 0.5, 1.0 and 5.0 μg/kg ranged from 85.6% to 105.2% with the RSD between 4.17% and 5.45%(n=6). The method was proved to be fast and effective for simultaneous qualitative and quantitative analysis of the metabolites of the nitrofuran antibiotics in chicken products.
作者
宋兴兴
SONG Xingxing(Inspection and Quarantine Technical Center, Suzhou Entry-Exit Inspection and Quarantine Bureau (Suzhou 215004);Suzhou Huabo Daily Chemicals Testing & Service Co., Ltd.(Suzhou 215104))
出处
《食品工业》
CAS
北大核心
2019年第1期308-310,共3页
The Food Industry
关键词
液相色谱-串联质谱法
鸡肉
硝基呋喃
代谢物
liquid chromatography-tandem mass spectrometry
chicken
nitrofuran
metabolites
